摘要
目的:建立气相色谱-质谱联用仪对蔬菜、水果中多种农药残留组分进行分析检测的方法。方法:取100g的果蔬样品,于组织捣碎机中打碎混匀后,称取10.0g,置于100mL离心管中,分别加入50mL的乙腈、5g的氯化钠,置于超声波振荡器中提取30min,静置,过滤。在此滤液中加入无水硫酸钠5g,震荡,在5000r/min条件下离心3min,分出乙腈25mL,用氮气吹干浓缩至约1.0mL,经弗罗里硅土固相萃取小柱进行净化,洗脱,用1mL的丙酮溶解定容,用0.45μm的滤膜进行过滤,供GC-MS分析用。结果:16种农药的最低检测浓度(LOD)为0.8~8.4μg/kg,平均回收率为85.3~108.2%。结论:本方法简便、快速、灵敏度及准确率高,能同时对蔬菜、水果中多种农药残留组分进行检测分析。
objective: To establish a method for determination of various components of pesticide residues in vegetables and fruits synchronously by gas chromatography-mass spectrometry.Method: 100g of fruits and vegetables samples were taken into the stamp mill series for shattering and blending. 10g samples were taken into the 100mL centrifuge tube, then 50mL acetonitrile,5g sodium chloride were added respectively. The centrifuge tube was placed in an ultrasonic oscillator for extraction about 30min,then Stewing and Filtering. 5g anhydrous sodium sulfate were added into the filtrate, then the samples were concussed, centrifugated in 5000 r/min for 3min to separate acetonitrile 25mL and dried by nitrogen and concentrated to about 1.0mL. The samples were purified and eluted by a Florisil SPE column.At last,1mL acetone were added to dissolve the sample and filtered with the 0.45 μ m filterable membrane for GC-MS analysis. Results: LOD of 16 pesticide residues were 0.8 ~8.4μg/kg, the average recovery was 85.3~108.2%. Conclusion: The method was handy, fast,sensitive, precise, and could detectvarious components of pesticide residuesin vegetables and fruits synchronously.
出处
《求医问药(下半月)》
2013年第10期46-47,共2页
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